X-ray reflectometry (XRR) is a well-known technique for measuring the thickness, density and surface quality of thin film layers deposited on a substrate. Conventional X-ray reflectometers are sold by a number of companies, among them Technos (Osaka, Japan), Siemens (Munich, Germany) and Bede Scientific Instrument (Durham, UK). Such reflectometers typically operate by irradiating a sample with a beam of X-rays at grazing incidence, i.e., at a small angle relative to the surface of the sample, near the total external reflection angle of the sample material. Measurement of X-ray intensity reflected from the sample as a function of angle gives a pattern of interference fringes, which is analyzed to determine the properties of the film layers responsible for creating the fringe pattern.
A method for analyzing the X-ray data to determine film thickness is described, for example, in U.S. Pat. No. 5,740,226, to Komiya et al., whose disclosure is incorporated herein by reference. After measuring X-ray reflectance as a function of angle, an average reflectance curve is fitted to the fringe spectrum. The average curve is based on a formula that expresses attenuation, background and surface roughness of the film. The fitted average reflectance curve is then used in extracting the oscillatory component of the fringe spectrum. This component is Fourier transformed to find the film thickness.
U.S. Pat. No. 5,619,548, to Koppel, whose disclosure is incorporated herein by reference, describes an X-ray thickness gauge based on reflectometric measurement. A curved, reflective X-ray monochromator is used to focus X-rays onto the surface of a sample. A position-sensitive detector, such as a photodiode detector array, senses the X-rays reflected from the surface and produces an intensity signal as a function of reflection angle. The angle-dependent signal is analyzed to determine properties of the structure of a thin film layer on the sample, including thickness, density and surface roughness.
U.S. Pat. No. 5,923,720, to Barton et al., whose disclosure is incorporated herein by reference, also describes an X-ray spectrometer based on a curved crystal monochromator. The monochromator has the shape of a tapered logarithmic spiral, which is described as achieving a finer focal spot on a sample surface than prior art monochromators. X-rays reflected or diffracted from the sample surface are received by a position-sensitive detector.
U.S. Pat. Nos. 6,512,814 and 6,639,968, to Yokhin et al., whose disclosures are incorporated herein by reference, describe an X-ray reflectometry system that includes a dynamic shutter, which is adjustably positionable to intercept the X-rays incident on the sample. This shutter, along with other features of the system, permits detection of XRR fringe patterns with high dynamic range. These patents also disclose improved methods for analysis of the XRR fringe pattern in order to determine thin film properties, including density, thickness and surface roughness. The high dynamic range enables the system to determine these properties accurately not only for the upper thin film layer, but also for one or more underlying layers on the surface of the sample.
Another common method of X-ray reflectometric measurement is described, for example, in an article by Naudon et al., entitled “New Apparatus for Grazing X-ray Reflectometry in the Angle-Resolved Dispersive Mode,” in Journal of Applied Crystallography 22 (1989), p. 460, which is incorporated herein by reference. A divergent beam of X-rays is directed toward the surface of a sample at grazing incidence, and a detector opposite the X-ray beam source collects reflected X-rays. A knife edge is placed close to the sample surface immediately above a measurement location in order to cut off the primary X-ray beam. A monochromator between the sample and the detector (rather than between the source and sample, as in U.S. Pat. No. 5,619,548) selects the wavelength of the reflected X-ray beam that is to reach the detector.
XRR may also be used in situ, within a deposition furnace, to inspect thin film layers in production on a semiconductor wafer, as described, for example, by Hayashi et al., in U.S. Patent Application Publication US 2001/0043668 A1, whose disclosure is incorporated herein by reference. The furnace is provided with X-ray incidence and extraction windows in its side walls. The substrate upon which the thin film has been deposited is irradiated through the incidence window, and the X-rays reflected from the substrate are sensed through the X-ray extraction window.
Whereas the references cited above are directed to measurement of specular X-ray reflections, diffuse X-ray reflections (alternatively referred to as diffuse scattering) can also provide surface information. Measurement of diffuse X-ray scattering is described, for example, by Stömmer in “X-ray Scattering from Silicon Surfaces,” in Semiconductor International (May 1, 1998), which is incorporated herein by reference. This article describes an experimental set-up in which a sample is irradiated by a collimated X-ray source, and scattered X-rays from the sample are received by a detector. The detector is positioned so that the sum of the angles of incidence and scattering is fixed at a total angle, which is denoted 2Θ. The sample is mounted on a goniometer, which permits the tilt angle of the sample (denoted Ω) to be varied relative to the incident beam, without changing the total angle 2Θ.
In this arrangement, the scattered X-ray signal received by the detector is measured as a function of the tilt angle Ω. A sharp specular peak is observed at Ω=Θ. Additional, diffuse reflection peaks are observed on both sides of the specular peak, at angles Ω=Φc and Ω=2Θ−Φc, wherein Φc is the critical angle for total external reflection from the sample. These diffuse reflection peaks were first observed by Yoneda, who described his findings in an article entitled “Anomalous Surface Reflection of X Rays,” Physical Review 131, pages 2010–2013 (1963), which is incorporated herein by reference. The peaks are therefore commonly referred to as “Yoneda wings.” As noted by Stömmer, the shape of the diffuse scattering curve is determined, inter alia, by the surface roughness of the sample, and the diffuse scattering measurements can be analyzed to determine surface properties.